Synthesis and Characterization of a Dumbbell-Shaped Polyrotaxane Based on Polytetrahydrofuran bis(3-aminopropyl) Terminated and α-Cyclodextrins Using Polyamidoamine (PAMAM) Dentrimers as Bulky Stoppers

2015 ◽  
Vol 1094 ◽  
pp. 41-48
Author(s):  
Ri Min Cong ◽  
Huai Qing Yu ◽  
Yan Gong Yang ◽  
Si Yi Yang ◽  
Jiao Li ◽  
...  
Keyword(s):  
Thermogravimetric Analysis ◽  
Inclusion Complex ◽  
Inclusion Complexes ◽  
Synthesis And Characterization ◽  
Wide Angle ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Channel Type

A dumbbell-shaped polyrotaxane based on polytetrahydrofuran bis (3-aminopropyl) terminated and α-cyclodextrins using polyamidoamine (PAMAM) dentrimers as bulky stoppers was successfully prepared. The1H NMR results show that the peaks of α-CDs in these polyrotaxanes are broadened compared with pure α-CDs. Wide-angle X-ray diffraction (XRD) measurements of the resulting polyrotaxanes suggest to produce a channel-type crystalline structure of inclusion complex. Thermogravimetric analysis (TGA) of the resultant polyrotaxanes show that α-CDs are significantly stabilized by the formation of the inclusion complexes.

Polypseudorotaxane Hydrogels Based on F127 Block-Selected Inclusion Complexation with α-Cyclodextrin

2012 ◽  
Vol 482-484 ◽  
pp. 1898-1903
Author(s):  
Ying Xue Zhou ◽  
Xiao Dong Fan ◽  
Dan Xue
Keyword(s):  
Thermal Stability ◽  
Inclusion Complex ◽  
Inclusion Complexation ◽  
Wide Angle ◽  
Acryloyl Chloride ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
Thermal Stability Of ◽  
Channel Type

Supramolecular hydrogels were formed through F127, acryloyl chloride modified F127 inclusion complex with α-cyclodextrin, respectively. The structure of modified copolymers and inclusion complex was characterized by Fourier transform infrared spectroscopy (FTIR) and hydrogen nuclear magnetic resonance (1H-NMR). Hydrogels formed from supramolecular inclusion are imparted channel-type structure investigated by wide angle x-ray diffraction (WAXRD). Differential scanning calorimetry (DSC) and TG experiments showed that thermal stability of hydrogels depend on the nature of axis polymer. The relative model was proposed to elucidate the inclusion complexes and hydrogels formation.

Synthesis and Electrochemistry of Aluminum Porphycenes: Crystal and Molecular Structure of Methyl-σ-Bonded Aluminum Etioporphycene

1997 ◽  
Vol 01 (02) ◽  
pp. 109-119 ◽  
Author(s):  
ROGER GUILARD ◽  
VIRGINIE PICHON-PESME ◽  
HASSANE LACHEKAR ◽  
CLAUDE LECOMTE ◽  
ALLY M. AUKAULOO ◽  
...  
Keyword(s):  
Molecular Structure ◽  
Crystal And Molecular Structure ◽  
Structural Data ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Axial Ligands ◽  
Uv Visible

The synthesis and characterization of three monomeric aluminum porphycenes with anionic or σ-bonded axial ligands is reported. The investigated compounds are represented as ( EtioPc ) Al ( CH 3) and ( EtioPc ) AlX where EtioPc represents the dianion of etioporphycene and X = Cl − or OH −. Each synthesized complex was characterized by mass spectrometry. 1 H NMR, IR and UV-visible spectroscopies as well as by electrochemistry. Comparisons are made between the properties of complexes in the aluminum etioporphycene series and related chloro- or methyl σ-bonded Al ( III ) porphyrins containing octaethylporphyrin ( OEP ) or tetraphenylporphyrin ( TPP ) macrocycles. Comparisons are also made between the currently investigated compounds and a previously reported Al ( III ) μ-oxo dimer, [( EtioPc ) Al ]2 O . In addition, the crystal and molecular structure of ( EtioPc ) Al ( CH 3) was determined by X-ray diffraction. The molecular structure of this methyl-σ-bonded aluminum etioporphycene provides the first structural data for an aluminum porphycene compound. The aluminum(III) atom in ( EtioPc ) Al ( CH 3) is pentacoordinated and is located 0.54 Å from the plane of the four N -nitrogens.

Synthesis and Characterization of Polythiophene / SBA-15 Composite

2014 ◽  
Vol 968 ◽  
pp. 49-52
Author(s):  
Qin Qin Hou
Keyword(s):  
Thermogravimetric Analysis ◽  
Oxidative Polymerization ◽  
Mesoporous Structure ◽  
Synthesis And Characterization ◽  
Scan Electron Micrographs ◽  
X Ray Diffraction ◽  
Channel System ◽  
X Ray ◽  
Adsorption Desorption

A new nanocomposite, semiconducting polythiophene (PT) confined in mesoporous silica (SBA-15) was synthesized. PT was formed in the pores of SBA-15 by subsequent oxidative polymerization with FeCl3. Different techniques were used to characterize the nanocomposite formation. X-ray diffraction (XRD) and N2 adsorption/desorption analysis showed that the nanocomposite possesses mesoporous structure, and the residual pore volume of nanocomposite was significantly lower than that of pure empty SBA-15. Scan electron micrographs confirmed the presence of polythiophene inside pore channels of the host, and thermogravimetric analysis proved confinement effect in the channel system.

Oxazoline chemistry — Part IV: Synthesis and characterization of oxazoline complexes of the zinc halides

2003 ◽  
Vol 81 (12) ◽  
pp. 1482-1491 ◽  
Author(s):  
Tosha M Barclay ◽  
Ignacio del Río ◽  
Robert A Gossage ◽  
Sarah M Jackson
Keyword(s):  
Crystal Structure ◽  
Structural Diversity ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
Metal Centre ◽  
Zinc Compounds ◽  
X Ray ◽  
H Nmr ◽  
Oxazoline Ligands

The synthesis and characterization of 11 zinc halide derivatives that contain monodentate oxazoline ligands is described. The treatment of ether solutions of [ZnX2] (X = Cl, Br, I) with 2-aryl- or 2-methyl-2-oxazolines results in the formation of mildly hygroscopic complexes of the general formulae [ZnX2(ox)2] (ox = 2-methyl-2-oxazoline (1), 2,4,4-trimethyl-2-oxazoline (2), 2-phenyl-2-oxazoline (3), or 4,4-dimethyl-2-phenyl-2-oxazoline (4)), except in the case of ZnI2, which does not form an isolable complex — likely for steric reasons — with oxazoline 4. Treatment of [ZnBr2(4)2] with 1 reveals (1H NMR) that 1 only sluggishly displaces coordinated 4 at temperatures below 50 °C. The structural characterization, via single crystal X-ray diffraction, of six of the complexes, viz. [ZnI2(1)2], [ZnI2(2)2], [ZnX2(3)2] (X = Cl, Br, or I), and [ZnBr2(4)2], is also reported. All of these structurally characterized complexes are mononuclear zinc compounds with an overall distorted tetrahedral arrangement of the two halide and two oxazoline ligands around the zinc metal centre. The oxazoline series of complexes reported herein show little structural diversity, a facet which is in contrast to their substituted pyridine analogues.Key words: oxazoline, zinc, X-ray crystal structure, coordination complex, NMR spectroscopy, Zn(II).

Synthesis and Characterization of Polyaniline Copolymer

2012 ◽  
Vol 217-219 ◽  
pp. 551-554
Author(s):  
Ting Xi Li ◽  
Yu Hua Zhao ◽  
Qian Li ◽  
Cheng Qian Yuan ◽  
Quan Liang Chen ◽  
...  
Keyword(s):  
Thermal Stability ◽  
Infrared Spectroscopy ◽  
Thermogravimetric Analysis ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
Ft Ir ◽  
The Difference ◽  
Thermal Stability Of

Abstract. Polyaniline (PANI) and p-phenylenediamine (p-PDA)-aniline copolymer were prepared via a same microemulsion method. The structures of the PANI and p-PDA-aniline copolymer were characterized by infrared spectroscopy (FT-IR), X-ray diffraction (XRD), thermogravimetric analysis（TGA）. The results revealed the difference of synthesis and characterization between PANI and p-PDA-aniline copolymer. It was shown that structure of the copolymer is almost similar to that of PANI, but the p-PDA-aniline copolymer has a better crystallization than PANI, and the thermal stability of the copolymer is higher than that of pure PANI.

Synthesis and characterization of a hexaphyrin(1.0.1.0.0.0) bearing both meso- and β-substituents

2007 ◽  
Vol 11 (04) ◽  
pp. 287-293 ◽  
Author(s):  
Jonathan L. Sessler ◽  
Patricia J. Melfi ◽  
Vincent M. Lynch
Keyword(s):  
Crystal Structure ◽  
Ring Current ◽  
Spectroscopic Studies ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Planar Conformation ◽  
Hydrogen Bound

The synthesis of an isoamethyrin-type expanded porphyrin bearing both meso- and β-substituents is presented. The diprotonated form of this macrocycle was characterized by conventional spectroscopic means and via a single crystal X-ray diffraction analysis. This species is observed to adopt a planar conformation in the solid state. Nonetheless, the inner ring current, as inferred from 1 H NMR spectroscopic studies, is found to be severely diminished as compared to isoamethyrin, by the presence of the two meso-phenyl moieties. A second crystal structure, in which a molecule of water is hydrogen-bound to a pyrrole NH , was also solved.

Synthesis and characterization of 2,2-diphenyl-1-(5-acetonyl-2,4,6-trinitro-1,3-cyclohexadienyl)hydrazine, C21H19N5O7

1993 ◽  
Vol 71 (7) ◽  
pp. 1057-1063 ◽  
Author(s):  
Donna L. Draper ◽  
Richard J. Barton ◽  
Beverly E. Robertson ◽  
Barbara R. Nelson ◽  
John A. Weil
Keyword(s):  
Nitro Group ◽  
Synthesis And Characterization ◽  
Boat Conformation ◽  
X Ray Diffraction ◽  
X Ray ◽  
H Nmr ◽  
Phenyl Rings ◽  
Common Plane ◽  
Twist Boat

The reaction of 2,2-diphenyl-1-(2,4,6-trinitrophenyl)hydrazine with the enolate of acetone, followed by acidification, yields the title compound 2,2-diphenyl-1-(5-acetonyl-2,4,6-trinitro-1,3-cyclohexadienyl)hydrazine, C21H19N5O7. The identity of the latter was confirmed by a combination of mass spectrometry, FTIR, elemental analysis, and 1H NMR. Crystals were grown from dichloromethane –95% ethanol and the structure was determined by X-ray diffraction. Crystals are monoclinic, P21/c, a = 9.254(3), b = 13.531(3), c = 17.39(5) Å, β = 106.18(2)° at 225 K. R = 0.073, Rω = 0.038 for reflections with I > 2σ(I). The Zachariasen extinction factor, g, refined to 18(3) × 10−4. The cyclohexadiene ring is puckered with a primarily twist-boat conformation. Atoms C(1) to C(3), C(6), the nitro group on C(2), and the hydrazine moiety (N(8)—N(7)—H(7) attached to C(1)) all lie close to a common plane. The planes of the two phenyl rings, the acetonyl substituent, and the C(6) nitro group are each roughly perpendicular to this plane. The C(5) acetonyl and C(6) nitro groups are trans to each other.

Preparation and Characterization of Tea Polyphenols/Starch Inclusion Complex

2013 ◽  
Vol 432 ◽  
pp. 413-417 ◽  
Author(s):  
Li Ming Zhang ◽  
Zhi Ying Hu ◽  
Li Hu Yan ◽  
Run Liu Li ◽  
Cheng Wei Cao ◽  
...  
Keyword(s):  
Differential Scanning Calorimetry ◽  
Inclusion Complex ◽  
Inclusion Complexes ◽  
Tea Polyphenols ◽  
X Ray Diffraction ◽  
Scanning Calorimetry ◽  
X Ray ◽  
The Stability ◽  
Good Retention

In order to improving the stability and bioavailability of tea polyphenols (TP), the TP/starchinclusion complex(TPSIC) was prepared by adding TP to starch slurry during gelatinization, and its TPreleasing behaviorswas investigated. The formation of inclusion complex was confirmed by powder X-ray diffraction (XRD) and differential scanning calorimetry (DSC). The TPSIC showed a characteristic of V-type crystallinity and a looser gel matrix. The encapsulation increased the stability of TP and generated a good releasing behavior after enzymatic erosion. The lower releasing rate indicated that the prepared inclusion complexes had good retention ability and effectively reduced the releasing rate of TP. The releasing rate of TPSIC increased with the increase of TP concentration.

Synthesis and Characterization of Novel Organomodified Nanoclays for Application in Dental Materials

2019 ◽  
Vol >15 (5) ◽  
pp. 512-524 ◽  
Author(s):  
Alexandros K. Nikolaidis ◽  
Elisabeth A. Koulaouzidou ◽  
Dimitris S. Achilias
Keyword(s):  
Fourier Transform ◽  
Infrared Spectroscopy ◽  
Thermogravimetric Analysis ◽  
Fourier Transform Infrared Spectroscopy ◽  
Quaternary Ammonium ◽  
Fourier Transform Infrared ◽  
Synthesis And Characterization ◽  
X Ray Diffraction ◽  
X Ray

Background: Nanoclays incorporated in dental resins have been previously investigated. However, limited reports are associated with nanoclays that exhibit high functionality. Objective: The aim of this study was the targeted synthesis and characterization of organomodified nanoclays with methacrylic groups suitable for incorporation in dental nanocomposite resins. Methods: Quaternary ammonium methacrylates were synthesized and characterized by means of proton nuclear magnetic resonance and Fourier-transform infrared spectroscopy. Consequently, they were inserted into the interlayer space of nanoclay through a cation exchange reaction, while silane was also used for simultaneous surface modification. The produced organomodified nanoclays were characterized by means of X-ray diffraction, Fourier-transform infrared spectroscopy and thermogravimetric analysis. Results: Fourier-transform infrared spectra confirmed the successful synthesis of the quaternary ammonium methacrylates. X-ray diffraction analysis showed that organoclays exhibited higher d001- values (up to 1.78 nm) compared to raw nanoclay (1.37 nm), indicating an accomplished intercalation in each case. X-ray diffraction spectra mainly disclosed the presence of methacrylic functional groups in all nanoclays. Thermogravimetric analysis curves verified the different thermal stability of organoclays due to the diversity of their organic modifiers. Conclusion: The experimental results showed that nanoclay was successfully modified with ammonium methacrylates and silane. Τhe combination of X-ray diffraction and thermogravimetric analysis data revealed a high degree of intercalation and methacrylated organic loading as well. These phenomena may favor a good dispersion and high polymerization degree of nanoclays with dental resin monomers, rendering them potentially useful materials for the development of advanced dental nanocomposites resins.

Synthesis and Characterization of Multi-Functional Substituted POSS

2012 ◽  
Vol 554-556 ◽  
pp. 227-230
Author(s):  
Li Ying Zhang ◽  
Xiao Jing Zhao ◽  
Ping Chen ◽  
Sheng Di Fan
Keyword(s):  
Thermal Stability ◽  
Nuclear Magnetic Resonance ◽  
Synthesis And Characterization ◽  
Wide Angle ◽  
X Ray Diffraction ◽  
X Ray ◽  
Good Thermal Stability ◽  
Elementary Analysis ◽  
Thermal Stability Of

Five different multifunctional nitro octaphenyl silsesquioxane (NPS) were Synthesised and reduction was carried out to obtain amino octaphenyl silsesquioxane(APS). These compounds were characterized with elementary analysis, fourier transform infrared(FTIR), nuclear magnetic resonance (NMR, 29Si), wide-angle X-ray diffraction(XRD) and thermogravimetry (TG). Experiental results showed that the longer the nitration time, the more nitro connected to the OPS, but not positively, nitro number remained unchanged after five hours. NPS has good thermal stability than corresponding APS under 450°C, and the thermal stability of APS are decrease with the increase of amino number.

Sign in / Sign up

Export Citation Format

Share Document